HRID540995
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
D-tryptophan methyl ester hydrochloride of Step 1 (100 g) and piperonal (65 g) were suspended in sulfolane (500 mL) at 25° C. to 30° C. The reaction mixture was heated to 80° C. to 85° C., stirred for 14 hours, and then cooled to 25° C. to 30° C. To the cooled mixture, dichloromethane (500 mL) was added and the resultant mixture was stirred continuously for 1 hour. The solid obtained was filtered, washed with dichloromethane (500 mL), and dried in air at 40° C. to 45° C. to afford cis 1-benzo[1,3]dioxol-5-yl-2,3,4,9-tetrahydro-1H-beta-carboline-3-carboxylic acid methyl ester hydrochloride.
WORKUP
后处理
- temperatureThe reaction mixture was heated to 80° C. to 85° C.
- temperaturecooled to 25° C. to 30° C
- customThe solid obtained
- filtrationwas filtered
- washwashed with dichloromethane (500 mL)
- customdried in air at 40° C. to 45° C.